CN108753221A - The preparation method and applications method of thermosetting property water-soluble urea-formaldehyde resin nano-powder adhesive - Google Patents
The preparation method and applications method of thermosetting property water-soluble urea-formaldehyde resin nano-powder adhesive Download PDFInfo
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- CN108753221A CN108753221A CN201810485983.0A CN201810485983A CN108753221A CN 108753221 A CN108753221 A CN 108753221A CN 201810485983 A CN201810485983 A CN 201810485983A CN 108753221 A CN108753221 A CN 108753221A
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- Prior art keywords
- formaldehyde resin
- thermosetting property
- adhesive
- soluble urea
- property water
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- 239000000853 adhesive Substances 0.000 title claims abstract description 88
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 88
- 229920001807 Urea-formaldehyde Polymers 0.000 title claims abstract description 58
- GZCGUPFRVQAUEE-SLPGGIOYSA-N aldehydo-D-glucose Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O GZCGUPFRVQAUEE-SLPGGIOYSA-N 0.000 title claims abstract description 56
- 239000011858 nanopowder Substances 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 41
- 229920001187 thermosetting polymer Polymers 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000002023 wood Substances 0.000 claims abstract description 59
- 230000029058 respiratory gaseous exchange Effects 0.000 claims abstract description 21
- 230000008569 process Effects 0.000 claims abstract description 17
- 229920005989 resin Polymers 0.000 claims abstract description 16
- 239000011347 resin Substances 0.000 claims abstract description 16
- 239000000758 substrate Substances 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 15
- 238000009777 vacuum freeze-drying Methods 0.000 claims abstract description 12
- 238000012216 screening Methods 0.000 claims abstract description 8
- 238000000227 grinding Methods 0.000 claims abstract description 7
- 238000003825 pressing Methods 0.000 claims abstract description 7
- 238000004519 manufacturing process Methods 0.000 claims description 13
- 239000000835 fiber Substances 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 10
- 238000004513 sizing Methods 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 7
- 230000015572 biosynthetic process Effects 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 238000012792 lyophilization process Methods 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 3
- 239000012267 brine Substances 0.000 claims description 2
- 238000009826 distribution Methods 0.000 claims description 2
- 239000003002 pH adjusting agent Substances 0.000 claims description 2
- 238000005057 refrigeration Methods 0.000 claims description 2
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims description 2
- 235000015110 jellies Nutrition 0.000 claims 1
- 239000008274 jelly Substances 0.000 claims 1
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 abstract description 45
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 14
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 238000005452 bending Methods 0.000 description 23
- 230000003068 static effect Effects 0.000 description 23
- 238000007731 hot pressing Methods 0.000 description 20
- 235000019256 formaldehyde Nutrition 0.000 description 19
- 239000000843 powder Substances 0.000 description 19
- 239000000463 material Substances 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 10
- 230000008961 swelling Effects 0.000 description 8
- 238000005470 impregnation Methods 0.000 description 7
- 230000000994 depressogenic effect Effects 0.000 description 6
- 238000004108 freeze drying Methods 0.000 description 6
- 230000006835 compression Effects 0.000 description 5
- 238000007906 compression Methods 0.000 description 5
- 239000012141 concentrate Substances 0.000 description 5
- 239000003292 glue Substances 0.000 description 5
- 238000004321 preservation Methods 0.000 description 5
- 238000010792 warming Methods 0.000 description 5
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 4
- 229960004279 formaldehyde Drugs 0.000 description 4
- 238000007711 solidification Methods 0.000 description 4
- 230000008023 solidification Effects 0.000 description 4
- 210000002268 wool Anatomy 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- HANVTCGOAROXMV-UHFFFAOYSA-N formaldehyde;1,3,5-triazine-2,4,6-triamine;urea Chemical compound O=C.NC(N)=O.NC1=NC(N)=NC(N)=N1 HANVTCGOAROXMV-UHFFFAOYSA-N 0.000 description 3
- 230000013011 mating Effects 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical class OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- 235000019270 ammonium chloride Nutrition 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 210000000988 bone and bone Anatomy 0.000 description 2
- 239000011093 chipboard Substances 0.000 description 2
- 239000011094 fiberboard Substances 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- ODGAOXROABLFNM-UHFFFAOYSA-N polynoxylin Chemical compound O=C.NC(N)=O ODGAOXROABLFNM-UHFFFAOYSA-N 0.000 description 2
- 238000001694 spray drying Methods 0.000 description 2
- 241000219000 Populus Species 0.000 description 1
- 238000010793 Steam injection (oil industry) Methods 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000007717 exclusion Effects 0.000 description 1
- 235000011194 food seasoning agent Nutrition 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000009688 liquid atomisation Methods 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 230000008542 thermal sensitivity Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J161/00—Adhesives based on condensation polymers of aldehydes or ketones; Adhesives based on derivatives of such polymers
- C09J161/20—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C09J161/22—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with acyclic or carbocyclic compounds
- C09J161/24—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with acyclic or carbocyclic compounds with urea or thiourea
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27D—WORKING VENEER OR PLYWOOD
- B27D1/00—Joining wood veneer with any material; Forming articles thereby; Preparatory processing of surfaces to be joined, e.g. scoring
- B27D1/04—Joining wood veneer with any material; Forming articles thereby; Preparatory processing of surfaces to be joined, e.g. scoring to produce plywood or articles made therefrom; Plywood sheets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27N—MANUFACTURE BY DRY PROCESSES OF ARTICLES, WITH OR WITHOUT ORGANIC BINDING AGENTS, MADE FROM PARTICLES OR FIBRES CONSISTING OF WOOD OR OTHER LIGNOCELLULOSIC OR LIKE ORGANIC MATERIAL
- B27N1/00—Pretreatment of moulding material
- B27N1/02—Mixing the material with binding agent
- B27N1/0209—Methods, e.g. characterised by the composition of the agent
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27N—MANUFACTURE BY DRY PROCESSES OF ARTICLES, WITH OR WITHOUT ORGANIC BINDING AGENTS, MADE FROM PARTICLES OR FIBRES CONSISTING OF WOOD OR OTHER LIGNOCELLULOSIC OR LIKE ORGANIC MATERIAL
- B27N3/00—Manufacture of substantially flat articles, e.g. boards, from particles or fibres
- B27N3/002—Manufacture of substantially flat articles, e.g. boards, from particles or fibres characterised by the type of binder
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27N—MANUFACTURE BY DRY PROCESSES OF ARTICLES, WITH OR WITHOUT ORGANIC BINDING AGENTS, MADE FROM PARTICLES OR FIBRES CONSISTING OF WOOD OR OTHER LIGNOCELLULOSIC OR LIKE ORGANIC MATERIAL
- B27N3/00—Manufacture of substantially flat articles, e.g. boards, from particles or fibres
- B27N3/02—Manufacture of substantially flat articles, e.g. boards, from particles or fibres from particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27N—MANUFACTURE BY DRY PROCESSES OF ARTICLES, WITH OR WITHOUT ORGANIC BINDING AGENTS, MADE FROM PARTICLES OR FIBRES CONSISTING OF WOOD OR OTHER LIGNOCELLULOSIC OR LIKE ORGANIC MATERIAL
- B27N3/00—Manufacture of substantially flat articles, e.g. boards, from particles or fibres
- B27N3/04—Manufacture of substantially flat articles, e.g. boards, from particles or fibres from fibres
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27N—MANUFACTURE BY DRY PROCESSES OF ARTICLES, WITH OR WITHOUT ORGANIC BINDING AGENTS, MADE FROM PARTICLES OR FIBRES CONSISTING OF WOOD OR OTHER LIGNOCELLULOSIC OR LIKE ORGANIC MATERIAL
- B27N3/00—Manufacture of substantially flat articles, e.g. boards, from particles or fibres
- B27N3/08—Moulding or pressing
- B27N3/18—Auxiliary operations, e.g. preheating, humidifying, cutting-off
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/12—Powdering or granulating
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2361/00—Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
- C08J2361/20—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08J2361/22—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with acyclic or carbocyclic compounds
- C08J2361/24—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with acyclic or carbocyclic compounds with urea or thiourea
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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Wood Science & Technology (AREA)
- Forests & Forestry (AREA)
- Organic Chemistry (AREA)
- Medicinal Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Polymers & Plastics (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Dry Formation Of Fiberboard And The Like (AREA)
Abstract
The present invention provides a kind of preparation method of thermosetting property water-soluble urea-formaldehyde resin nano-powder adhesive, includes the following steps：Step 1, the vacuum concentration of thermosetting property water-soluble urea-formaldehyde resin adhesive；Step 2 carries out pH value adjustment to the thermosetting property water-soluble urea-formaldehyde resin adhesive after concentration；Step 3 carries out the thermosetting property water-soluble urea-formaldehyde resin adhesive after pH value adjustment to step 2 and carries out vacuum freeze drying；Step 4, grinding and screening after vacuum freeze drying.Adhesive prepared by this method is used to be applied to high-moisture percentage artificial board substrate with dry method resin application methods, the hot pre-pressing process of type of respiration produces wood-based plate, artificial board substrate's energy consumption for drying can be reduced, curing rate, bonding strength and the water resistance of adhesive are improved, reduces artificial board formaldehyde burst size.
Description
Technical field
The present invention relates to a kind of preparation method of thermosetting property water-soluble urea-formaldehyde resin nano-powder adhesive and its artificial
Application process in plate production, belongs to wood-based plate manufacturing field.
Background technology
The yield of China's wood-based plate in 2015 accounts for the 60% of world's wood-based plate yield up to 2.87 billion cubic meters, consumes adhesive
15300000 tons, consumption is still increased in the increase with wood-based plate yield with 10% or so speed.Wherein urea-formaldehyde resin adhesive
Consumption is 13,920,000 tons（Adhesive containing Urea-melamine-formaldehyde co-condensed resin）, it is close to account for Artificial Plate Adhesive consumption
90%.Urea-formaldehyde resin adhesive is the cheapest kind of price in all synthetic resin, is occupied in Wood-based Panel Production for a long time leading
Status will can not be replaced within considerable time by other adhesives.But it is there are Form aldehyde release, poor water resistance and to being glued
Substrate moisture rate requires low defect, long-standing problem wood-based panel industry circle.
General spray drying is a kind of suspended particles processing technology, is that feed liquid atomization is become tiny mist using high pressure
It drips, and evaporates the process of solvent formation power-product rapidly in heated drying medium.The drying means can make thermosensitive type liquid glue
Glutinous agent continues polycondensation during heating, and molecular weight is caused to increase, and physicochemical properties change, while the powder after drying
Surface is hardened, and leads to dry powder grinding and again dissolving difficulty, and then influence glue performance.
What the solidification of urea-formaldehyde resin adhesive typically carried out in acid condition, be generally by ureaformaldehyde in wood-based panel industry
The pH value of Resin adhesive uses between being adjusted to 3 ~ 5, to reach quick-setting purpose.Too low pH value makes solidification when impregnation
The excessive acid of remaining in system, and excessive acid can be such that the hydrolysis rate of solidified resin accelerates, and cause urea-formaldehyde resin adhesive resistance to
Aqueous difference, to influence the performance of wood-based plate, when impregnation, higher pH value was conducive to improve the water resistance of urea-formaldehyde resin adhesive.
In order to obtain ideal bonding strength, urea-formaldehyde resin adhesive has the relative moisture content of artificial board substrate when curing
It is strict with, base material relative moisture content is generally between 8 ~ 10%, at most no more than 12%, in order to which the control of substrate moisture rate exists
In the range of regulation, the drying for consuming a large amount of energy for artificial board substrate is needed.It is produced using high-moisture percentage base material artificial
Plate, to energy-saving, reduction Wood-based Panel Production cost, great meaning.It is limited to contain base material when urea-formaldehyde resin adhesive solidification
The requirement of water rate realizes that the splicing of high-moisture percentage base material needs new technical measures.
Patent CN107325765A provides a kind of spray drying preparation of melamine-formaldehyde-urea adhesive
And Wood composite preparation method for material, it is dry after powder without nanosizing milled processed, when use, need to be dissolved in water, and base material contains
Water rate 8% hereinafter, using wet method resin application methods, conventional pre-pressing process.
Patent of invention CN104493948B provides a kind of preparation method of high-moisture percentage particieboard, and the moisture content of wood shavings is
20 ~ 40%, using liquid resin application methods, resin added is 5 ~ 8%, conventional pre-pressing process, and adhesive used is that blocked polyurethane is pre-
Adhesive is blended with melamine-urea formaldehyde in aggressiveness.
It is the method using electrostatic atomization that patent of invention CN103737695B, which provides a kind of dry method glue applying method, by dry powder
It is applied in high-moisture percentage wood shavings, fiber, the dry powder composition is extremely complex, is micron order, using conventional pre-pressing process.
Invention content
The present invention provides a kind of thermosetting property water solubility urea to solve drawbacks described above and deficiency existing in the prior art
The preparation method of urea formaldehyde nano-powder adhesive and its application process in Wood-based Panel Production, include the following steps：
Step 1, the vacuum concentration of thermosetting property water-soluble urea-formaldehyde resin adhesive；
Step 2 carries out pH value adjustment to the thermosetting property water-soluble urea-formaldehyde resin adhesive after concentration；
It is dry to carry out the thermosetting property water-soluble urea-formaldehyde resin adhesive progress vacuum refrigeration after pH value adjustment to step 2 for step 3
It is dry；
Step 4, to through vacuum freeze drying, treated that thermosetting property water-soluble urea-formaldehyde resin adhesive is ground and sieves,
Obtain thermosetting property water-soluble urea-formaldehyde resin nano-powder adhesive.
Wherein, in step 1, the vacuum concentration condition of thermosetting property water-soluble urea-formaldehyde resin adhesive is：Vacuum degree is 0.05
~ 0.09MPa, temperature concentrated in vacuo are 20 ~ 50 DEG C, and the solid content after concentration is between 50 ~ 80%.
In step 2, for the pH value after adjustment between 5 ~ 7, pH adjusting agent is dilute acid solution or acid brine solution.
In step 3, vacuum freeze drying is divided into precooling process, lyophilization process and parsing drying process；Wherein,
The temperature of precooling process is less than -40 DEG C, and the vacuum degree of lyophilization process is 0.01 ~ 0.1mbar, freeze temperature is -40
~ -60 DEG C, the vacuum degree of parsing-desiccation process is 0.001 ~ 0.01mbar, freeze temperature -60 ~ -80 DEG C.
In step 4, grinding uses nanon ball-mill, and grinding temperature is between 80 ~ 250 DEG C；Particle size distribution range after screening
Between 400 ~ 900nm.
The present invention also provides a kind of thermosetting property water-soluble urea-formaldehyde resin nano-powder adhesives prepared using the above method
Application in Wood-based Panel Production, it is characterised in that include the following steps：
Step 1 is glued wood-based plate by the way of dry method sizing；
Step 2, artificial board substrate after sizing through mat formation or assembly after carry out the hot precompressed of type of respiration.
Further, sizing object is wood shavings layer, fibrous layer or veneer layer in artificial board substrate, the wood shavings layer, fibrous layer
And the relative moisture content of veneer layer is between 30 ~ 100%.
Further, in step 1, Lauxite nano-powder adhesive is applied to wood shavings layer in such a way that air-flow blows and spreads
Or fiber layer surface, continuous mechanical agitation, resin added are the 5 ~ 20% of wood shavings layer or fibrous layer absolute dry weight；Or Lauxite
Adhesive nano-powder is applied to the surface of veneer layer in such a way that air-flow blows and spreads, and resin added is 50 ~ 100g/m2。
Further, in step 2, the hot precompressed of type of respiration refers to being kept the temperature after hot press is increased to assigned temperature, by wood-based plate
Slab is placed in hot press and opens after shelves slowly boost to specified unit pressure pressurize for a period of time, slowly unloads and is pressed onto specified unit pressure
Pressurize is for a period of time again afterwards.A boosting ~ pressurize ~ release ~ dwell period is often undergone, breathing 1 time is denoted as.
Further, in step 2, precompressed unit pressure is between 0 ~ 5MPa, and precompressed temperature is between 110 ~ 180 DEG C, breathing
Number is more than 3 times.
The advantageous effects that the present invention is reached：
A kind of preparation method of thermosetting property water-soluble urea-formaldehyde resin nano-powder adhesive provided by the invention, vacuum freeze drying
It carries out at low temperature, especially suitable for thermal sensitivity, such as the drying of Thermosetting adhesive, molecular weight of material and physical chemistry after drying
Property is consistent with before drying, short texture, is in spongy, dissolves rapid and complete, property before meeting restores to freeze-drying at once after meeting water
Shape packs after the glutinous agent of Lauxite is freeze-dried, and Storage period was up to 1 year or more.
Lauxite nano-powder adhesive, the Mechanochemistry in high temperature and process of lapping are prepared by hot lapping mode
Free formaldehyde volatilization remaining in urea-formaldehyde resin powder and ether bond rupture can be promoted to release formaldehyde.Through high temperature and milled processed
Lauxite application of nanopowder when Wood-based Panel Production, burst size of methanal can be significantly reduced.
Using adhesive prepared by this method, nanometer grade powder has high specific surface area for nanometer grade powder, is tool
The physical basis for having superpower adsorption effect, the Lauxite nano-powder adhesive prepared using the method is from artificial board substrate
It adsorbs large quantity of moisture and dissolves and soak base material；Containing a large amount of unreacted in dissolved Lauxite nano-powder adhesive
Moisture and cellulose in methylol, with artificial board substrate form hydrogen bond, substantially increase Lauxite nano-powder adhesive
Pre-pressure property.
Dry method resin application methods are applied to high-moisture percentage artificial board substrate, and dry method is glued, and moisture-free in adhesive will not be led
Substrate moisture rate is caused to improve；And dissolving is needed to need to draw from base material to obtain wetability and mobility before adhesive solidification
Moisture, therefore base material must have higher relative moisture content, just contain when more than fibre saturated point, in base material and be easy to be inhaled
Attached Free water, thus artificial board substrate's unit only need it is dry to compared with high-moisture percentage or being not required to dry can be used to wood-based plate life
Production.Dry method is glued, and adhesive has 100% solid content, saves the moisture evaporation time in adhesive, and hardening time significantly shortens；
The solid content positive correlation of bonding strength and adhesive after powder dissolving remains to that the solid being glued far beyond wet method is kept to contain
Amount, bonding strength significantly improve.
Using hot prestressing technology, the moisture rapid vaporization in base material can be made, steam injection pressing effect is formed, be plasticized plate rapidly
Base reduces slab thickness；Promote the dissolving of nano-powder adhesive and precuring simultaneously, further increases Pre-pressure property.Using exhaling
Suction precompressed can promote formaldehyde newly-generated in still remaining free formaldehyde, procuring process after high temperature grinding with high pressure water
Discharge is forced in the exclusion of steam, further decreases the burst size of methanal of wood-based plate.
When being hot pressed into plate using conventional hot-press technique, since dissolved adhesive has higher pH value, glue-line is not
Facile hydrolysis, water resistance significantly improve.
The present invention is glued by nano-powder adhesive dry method in high-moisture percentage base material, is given birth to using the hot pre-pressing process of type of respiration
Wood-based plate is produced, artificial board substrate's unit energy consumption for drying can be reduced, shortens adhesive hardening time, improves wood-based plate bonding strength
And water resistance, reduce burst size of methanal.
Specific implementation mode
With reference to specific embodiment, the invention will be further described.Following embodiment is only used for clearly illustrating
Technical scheme of the present invention, and not intended to limit the protection scope of the present invention.
Patent of the present invention is further illustrated with reference to embodiment.
Embodiment 1
Thermosetting property water-soluble urea-formaldehyde resin is concentrated at vacuum degree 0.05MPa, the temperature of adhesive is controlled at 20 DEG C when concentration,
It is concentrated into solid content 50%, pH value is adjusted to vacuum freeze drying after 5 with 20% phosphate aqueous solution.Concentrate is in -40 DEG C of pre-freezes
To complete ice knot；Lyophilization section, vacuum degree 0.01mbar, -40 DEG C of freeze temperature；Parsing-desiccation section, vacuum degree
0.001mbar, freeze temperature obtain dry powder at -80 DEG C.Dry powder is ground through nanon ball-mill at 80 DEG C, is ground to screening value
400nm obtains nano-powder.Nano-powder is applied in such a way that air-flow blows and spreads in wood-fibred, and nano-powder is with wood-fibred through machine
Tool is uniformly mixed, and it is 30% that wood-fibred, which is dried to relative moisture content, and the applied amount of nano-powder is in terms of bone dry fiber quality 5%
It calculates.Fiber sizing enters hot press precompressed after mating formation, hot press is warming up to 110 DEG C, heat preservation.The hot precompressed curve of slab is slowly to rise
It is depressed into unit pressure 5MPa, after pressurize 5min, slowly unloads and be depressed into unit pressure 0 MPa, pressurize 5min, be denoted as breathing 1 time, continuously
Thorough release after breathing 3 times.Slab immediately enters another 1 hot press hot pressing, 180 DEG C of hot pressing temperature, hot pressing unit pressure after release
2MPa, hot pressing time 1min/mm.Embodiment result：Indoor type medium density fibre board (MDF), density 0.65kg/m3, plate thickness 8mm, interior glue
Close 0.71 MPa of intensity, 25.2 MPa of static bending strength, 2850 MPa of elasticity modulus, 1.3 MPa of surface bonding intensity, water sucting thickness
Expansion rate 12.8%, burst size of methanal 5.4mg/100g.
Comparative example：Using commercially available common urea-formaldehyde resin adhesive, wood-fibred moisture content is dried to 8%, impregnation mode and
Resin added is identical as implementation column 1, conventional precompressed mode, and hot compression parameters are same as Example 1.Comparative example result：Indoor type
Medium density fibre board (MDF), density 0.65kg/m3, plate thickness 8mm, 0.31 MPa of interior bonding strength, 18.5 MPa of static bending strength, springform
Measure 2430 MPa, 0.7 MPa of surface bonding intensity, thickness swelling rate 18.8%, burst size of methanal 15.4mg/100g.
As can be seen from the comparison result, the wood-based plate produced using common urea-formaldehyde resin adhesive, interior bonding strength,
Static bending strength, elasticity modulus and surface bonding intensity are below in embodiment 1 to be produced using Lauxite nano-powder adhesive
The wood-based plate gone out；And thickness swelling rate and burst size of methanal are more than embodiment 1.
Embodiment 2
Thermosetting property water-soluble urea-formaldehyde resin is concentrated at vacuum degree 0.06MPa, the temperature of adhesive is controlled at 30 DEG C when concentration,
It is concentrated into solid content 60%, pH value is adjusted to vacuum freeze drying after 7 with 20% phosphate aqueous solution.Concentrate is in -45 DEG C of pre-freezes
To complete ice knot；Lyophilization section, vacuum degree 0.02mbar, -45 DEG C of freeze temperature；Parsing-desiccation section, vacuum degree
0.002mbar, freeze temperature obtain dry powder at -70 DEG C.Dry powder is ground through nanon ball-mill at 250 DEG C, is ground to screening value
900nm obtains nano-powder.Nano-powder is applied in such a way that air-flow blows and spreads in wood-fibred, and nano-powder is with wood-fibred through machine
Tool is uniformly mixed, and it is 100% that wood-fibred, which is dried to relative moisture content, and the applied amount of nano-powder is with bone dry fiber quality 20%
It calculates.Fiber sizing enters hot press precompressed after mating formation, hot press is warming up to 180 DEG C, heat preservation.The hot precompressed curve of slab is slow
It boosts to unit pressure 5MPa, after pressurize 5min, slowly unloads and be depressed into unit pressure 0 MPa, pressurize 5min, be denoted as breathing 1 time, even
Thoroughly slab immediately enters another 1 hot press hot pressing, 200 DEG C of hot pressing temperature, hot pressing unit pressure after release release after continuous breathing 5 times
2.5MPa, hot pressing time 1.5min/mm.Embodiment result：Plain edition high density fiberboard, density 0.85kg/m3, plate thickness 8mm,
0.91 MPa of interior bonding strength, 38.2 MPa of static bending strength, 3850 MPa of elasticity modulus, 1.3 MPa of surface bonding intensity, water suction
Thickness swelling 12.8%, burst size of methanal 6.1mg/100g.
Comparative example：Using commercially available common urea-formaldehyde resin adhesive, wood-fibred moisture content is dried to 8%, impregnation mode and
Resin added is identical as implementation column 2, conventional precompressed mode, and hot compression parameters are same as Example 2.Comparative example result：Plain edition
High density fiberboard, density 0.85kg/m3, plate thickness 8mm, 0.51 MPa of interior bonding strength, 32.2 MPa of static bending strength, springform
Measure 3250 MPa, 0.85 MPa of surface bonding intensity, thickness swelling rate 19.8%, burst size of methanal 16.4mg/100g.
As can be seen from the comparison result, the wood-based plate produced using common urea-formaldehyde resin adhesive, interior bonding strength,
Static bending strength, elasticity modulus and surface bonding intensity are below in embodiment 2 to be produced using Lauxite nano-powder adhesive
The wood-based plate gone out；And thickness swelling rate and burst size of methanal are more than embodiment 2.
Embodiment 3
Thermosetting property water-soluble urea-formaldehyde resin is concentrated at vacuum degree 0.07MPa, the temperature of adhesive is controlled at 40 DEG C when concentration,
It is concentrated into solid content 70%, pH value is adjusted to vacuum freeze drying after 5.5 with 20% ammonium sulfate solution.Concentrate is at -50 DEG C
Pre-freeze is to complete ice knot；Lyophilization section, vacuum degree 0.03mbar, -50 DEG C of freeze temperature；Parsing-desiccation section, vacuum degree
0.003mbar, freeze temperature obtain dry powder at -60 DEG C.Dry powder is ground through nanon ball-mill at 100 DEG C, is ground to screening value
700nm obtains nano-powder.Nano-powder is applied in such a way that air-flow blows and spreads in wood wool, and nano-powder is with wood wool through machine
Tool is uniformly mixed, and it is 40% that wood wool, which is dried to relative moisture content, and the applied amount of nano-powder is with over dry wood shavings quality 15%
It calculates.Sizing wood shavings enter hot press precompressed after mating formation, hot press is warming up to 140 DEG C, heat preservation.The hot precompressed curve of slab is slow
It boosts to unit pressure 2.5MPa, after pressurize 5min, slowly unloads and be depressed into unit pressure 0.5 MPa, pressurize 5min and be denoted as breathing 1
It is secondary, thorough release after continuously breathing 4 times.Slab immediately enters another 1 hot press hot pressing, 190 DEG C of hot pressing temperature, hot pressing list after release
Position pressure 2.5MPa, hot pressing time 1.5min/mm.Embodiment result：The common shaving board used under drying regime, density
0.55kg/m3, plate thickness 9mm, 0.41 MPa of interior bonding strength, 11.2 MPa of static bending strength.
Comparative example：Using commercially available common urea-formaldehyde resin adhesive, wood wool moisture content is dried to 8%, impregnation mode and
Resin added is identical as implementation column 3, conventional precompressed mode, and hot compression parameters are same as Example 3.Comparative example result：Dry shape
The common shaving board used under state, density 0.55kg/m3, plate thickness 9mm, 0.32 MPa of interior bonding strength, static bending strength 8.2
MPa。
As can be seen from the comparison result, the wood-based plate produced using common urea-formaldehyde resin adhesive, interior bonding strength
It is below the wood-based plate produced using Lauxite nano-powder adhesive in embodiment 3 with static bending strength.
Embodiment 4
Thermosetting property water-soluble urea-formaldehyde resin is concentrated at vacuum degree 0.08MPa, the temperature of adhesive is controlled at 50 DEG C when concentration,
It is concentrated into solid content 80%, pH value is adjusted to vacuum freeze drying after 6 with 20% aqueous ammonium chloride solution.Concentrate is pre- at -60 DEG C
Freeze to complete ice knot；Lyophilization section, vacuum degree 0.04mbar, -55 DEG C of freeze temperature；Parsing-desiccation section, vacuum degree
0.004mbar, freeze temperature obtain dry powder at -55 DEG C.Dry powder is ground through nanon ball-mill at 90 DEG C, is ground to screening value
600nm obtains nano-powder.Nano-powder is applied in such a way that air-flow blows and spreads on strip wood shavings, nano-powder and strip wood shavings
It is uniformly mixed through mechanical agitation, strip particle drying to relative moisture content is 60%, and the applied amount of nano-powder is with over dry wood shavings matter
Amount 18% calculates.Enter hot press precompressed after being glued strip wood shavings orienting spreading, hot press is warming up to 150 DEG C, heat preservation.Slab heat
Precompressed curve is slowly to boost to unit pressure 3.0MPa, after pressurize 6min, slowly unloads and is depressed into 0.5 MPa of unit pressure, pressurize
6min is denoted as breathing 1 time, thorough release after continuously breathing 3 times.Slab immediately enters another 1 hot press hot pressing, hot pressing temperature after release
190 DEG C of degree, hot pressing unit pressure 2.5MPa, hot pressing time 1.5min/mm.Embodiment result：It is used under indoor seasoning state
General service oriented wood chipboard, density 0.65kg/m3, plate thickness 8mm, 0.61 MPa of interior bonding strength, parallel static bending strength 22.2
MPa, 11.5 MPa of vertical static bending strength, 2850 MPa of the parallel modulus of elasticity in static bending, 1300 MPa of vertical curve elasticity modulus,
Thickness swelling rate 22.8% for 24 hours, burst size of methanal 6.5mg/100g.
Comparative example：Using commercially available common urea-formaldehyde resin adhesive, strip wood shavings moisture content is dried to 8%, impregnation mode
Identical as implementation column 4 with resin added, conventional precompressed mode, hot compression parameters are same as Example 4.Comparative example result：It is indoor
The general service oriented wood chipboard used under drying regime, density 0.65kg/m3, plate thickness 8mm, 0.51 MPa of interior bonding strength,
18.2 MPa of parallel static bending strength, 9.4 MPa of vertical static bending strength, 2140 MPa of the parallel modulus of elasticity in static bending, vertical curve bullet
Property 1100 MPa of modulus, for 24 hours thickness swelling rate 19.2%, burst size of methanal 13.2mg/100g.
As can be seen from the comparison result, the wood-based plate produced using common urea-formaldehyde resin adhesive, interior bonding strength,
Parallel static bending strength, vertical static bending strength, parallel perfect elasticity modulus and vertical curve elasticity modulus are below in embodiment 4 and adopt
The wood-based plate that agent is produced is sticked with urea-formaldehyde resin adhesive nano-powder；And thickness swelling rate and burst size of methanal are more than embodiment
4。
Embodiment 5
Thermosetting property water-soluble urea-formaldehyde resin is concentrated at vacuum degree 0.09MPa, the temperature of adhesive is controlled at 45 DEG C when concentration,
It is concentrated into solid content 75%, pH value is adjusted to vacuum freeze drying after 6 with 20% aqueous ammonium chloride solution.Concentrate is pre- at -55 DEG C
Freeze to complete ice knot；Lyophilization section, vacuum degree 0.05mbar, -55 DEG C of freeze temperature；Parsing-desiccation section, vacuum degree
0.005mbar, freeze temperature obtain dry powder at -60 DEG C.Dry powder is ground through nanon ball-mill at 150 DEG C, is ground to screening value
800nm obtains nano-powder.Nano-powder is uniformly applied on board using poplar board in such a way that air-flow blows and spreads, and veneer is real without drying
Border relative moisture content is 60%, and the applied amount of nano-powder is with 50g/m2It calculates.It is pre- to enter hot press after the sizing normal assembly of veneer
Pressure, hot press are warming up to 140 DEG C, heat preservation.The hot precompressed curve of slab is slowly to boost to unit pressure 1.5MPa, pressurize 3min
Afterwards, it slowly unloads and is depressed into unit pressure 0.2 MPa, pressurize 3min, be denoted as breathing 1 time, thorough release after continuously breathing 4 times.Release
Slab immediately enters another 1 hot press hot pressing, 120 DEG C of hot pressing temperature, hot pressing unit pressure 1.0MPa, hot pressing time 1.0min/ afterwards
mm.Embodiment result：Common II class glued boards, plate thickness 10mm, 0.75 MPa of bonding strength, 29.2 MPa of rift grain static bending strength,
17.5 MPa of band static bending strength, 5200 MPa of modulus of elasticity parellel to grain, 2700 MPa of tangential elastic module, burst size of methanal
5.5mg/L。
Comparative example：Using commercially available common urea-formaldehyde resin adhesive, Veneer moisture is dried to 8%, impregnation mode and is applied
Glue amount is identical as implementation column 5, conventional precompressed mode, and hot compression parameters are same as Example 5.Comparative example result：Common II classes
Glued board, plate thickness 10mm, 0.71 MPa of bonding strength, 24.1 MPa of rift grain static bending strength, band static bending strength 15.2 MPa are suitable
4900 MPa of line elasticity modulus, tangential elastic module 2450 MPa, burst size of methanal 13.5mg/L.
As can be seen from the comparison result, the wood-based plate produced using common urea-formaldehyde resin adhesive, it is bonding strength, suitable
Line static bending strength, band static bending strength, modulus of elasticity parellel to grain and tangential elastic module, which are below in embodiment 5, uses Lauxite
The wood-based plate that nano-powder adhesive is produced；And burst size of methanal is more than embodiment 5.
The present invention is disclosed with preferred embodiment above, so it is not intended to limiting the invention, all to take equivalent replacement
Or the technical solution that the scheme of equivalent transformation is obtained, it all falls in protection scope of the present invention.
Claims (10)
1. a kind of preparation method of thermosetting property water-soluble urea-formaldehyde resin nano-powder adhesive, it is characterised in that including following step
Suddenly：
Step 1, the vacuum concentration of thermosetting property water-soluble urea-formaldehyde resin adhesive；
Step 2 carries out pH value adjustment to the thermosetting property water-soluble urea-formaldehyde resin adhesive after concentration；
It is dry to carry out the thermosetting property water-soluble urea-formaldehyde resin adhesive progress vacuum refrigeration after pH value adjustment to step 2 for step 3
It is dry；
Step 4, to through vacuum freeze drying, treated that thermosetting property water-soluble urea-formaldehyde resin adhesive is ground and sieves,
Obtain thermosetting property water-soluble urea-formaldehyde resin nano-powder adhesive.
2. the preparation method of thermosetting property water-soluble urea-formaldehyde resin nano-powder adhesive according to claim 1, feature
It is：In step 1, the vacuum concentration condition of thermosetting property water-soluble urea-formaldehyde resin adhesive is：Vacuum degree be 0.05 ~
0.09MPa, temperature concentrated in vacuo are 20 ~ 50 DEG C, and the solid content after concentration is between 50 ~ 80%.
3. the preparation method of thermosetting property water-soluble urea-formaldehyde resin nano-powder adhesive according to claim 1, feature
It is：In step 2, for the pH value after adjustment between 5 ~ 7, pH adjusting agent is dilute acid solution or acid brine solution.
4. the preparation method of thermosetting property water-soluble urea-formaldehyde resin nano-powder adhesive according to claim 1, feature
It is：In step 3, vacuum freeze drying is divided into precooling process, lyophilization process and parsing drying process；Wherein, it is pre-chilled
The temperature of jelly process is less than -40 DEG C, and the vacuum degree of lyophilization process is 0.01 ~ 0.1mbar, freeze temperature is -40 ~ -60
DEG C, the vacuum degree of parsing-desiccation process is 0.001 ~ 0.01mbar, freeze temperature -60 ~ -80 DEG C.
5. the preparation method of thermosetting property water-soluble urea-formaldehyde resin nano-powder adhesive according to claim 1, feature
It is：In step 4, grinding uses nanon ball-mill, and grinding temperature is between 80 ~ 250 DEG C；Particle size distribution range exists after screening
Between 400 ~ 900nm.
6. the thermosetting property water-soluble urea-formaldehyde resin nano-powder adhesive prepared using the method for any one of claim 1 ~ 5 is in people
Make the application in plate production, it is characterised in that include the following steps：
Step 1 is glued wood-based plate by the way of dry method sizing；
Step 2, artificial board substrate after sizing through mat formation or assembly after carry out the hot precompressed of type of respiration.
7. thermosetting property water-soluble urea-formaldehyde resin nano-powder adhesive answering in Wood-based Panel Production according to claim 6
With, it is characterised in that：Be glued object be artificial board substrate in wood shavings layer, fibrous layer or veneer layer, the wood shavings layer, fibrous layer and
The relative moisture content of veneer layer is between 30 ~ 100%.
8. thermosetting property water-soluble urea-formaldehyde resin nano-powder adhesive answering in Wood-based Panel Production according to claim 6
With, it is characterised in that：In step 1, Lauxite nano-powder adhesive be applied in such a way that air-flow blows and spreads wood shavings layer or
Fiber layer surface, and mechanical agitation is uniform, resin added is the 5 ~ 20% of wood shavings layer or fibrous layer absolute dry weight；Or urea-formaldehyde resin adhesive
Glutinous agent nano-powder is uniformly applied to the surface of veneer layer in such a way that air-flow blows and spreads, and resin added is in 50 ~ 100g/m2Between.
9. thermosetting property water-soluble urea-formaldehyde resin nano-powder adhesive answering in Wood-based Panel Production according to claim 6
With, it is characterised in that：In step 2, the hot precompressed of type of respiration refers to being kept the temperature after hot press is increased to assigned temperature, by wood-based plate
Slab is placed in hot press and opens after shelves slowly boost to specified unit pressure pressurize for a period of time, slowly unloads and is pressed onto specified unit pressure
Pressurize for a period of time, often undergoes the period of a boosting ~ pressurize ~ release ~ pressurize again afterwards, is denoted as breathing 1 time.
10. thermosetting property water-soluble urea-formaldehyde resin nano-powder adhesive according to claim 9 is in Wood-based Panel Production
Using, it is characterised in that：The hot pre-pressing process parameter of type of respiration is that precompressed unit pressure is between 0 ~ 5MPa, and precompressed temperature is 110
Between ~ 180 DEG C, respiration rate is more than 3 times.
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Cited By (1)
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| US11958942B1 (en) * | 2023-04-10 | 2024-04-16 | Southwest Forestry University | Method for recycling urea-formaldehyde (UF) and raw materials from wood-based panel, and use thereof |
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